2,3,7,8,12,13,17,18-八乙基-21H,23H-卟吩钯(II)合成路线 (共 2 条)
反应条件
in further solvent(s) dissolving of 2,3,7,8,12,13,17,18-octaethylporphine and PdCl2 in molar ratio of 1:10 in DMF; reflux for 2 min; cooling, pptn., filtration, pouring into H2O; pptn., filtation, washing with H2O, chromy. on silica gel (CHCl3:C6H12 (1:2) as eluent); elem. anal.;
参考文献
Chizhova; Mamardashvili
Russian Journal of Inorganic Chemistry, 2007 , vol. 52, # 2 p. 250 - 253
反应条件
in methanol; chloroform (N2 or Ar atmosphere); solid Pd(C2H3O2)2 is added to a soln. of H2(OEC) in CHCl3 and MeOH, stirred soln. is heated in a bath of boiling H2O, react. is monitored by TLC and UV-vis spectroscopy, color of soln. becomes deep blue within 15 min; soln. is taken to dryness, residue is purified by chromy. on silica gel, elution (hexane/toluene) gives a blue band (Pd(OEC)) followed by an orange-pink one (Pd(OEP)), solid recovered from the pure Pd(OEC) band is recrystd. from CHCl3/MeOH.;
参考文献
Inorganic Chemistry, , vol. 30, p. 3205 - 3213